Sodium Hydroxide → 2-[1-[3'-(1-Methyl-3-pentylureido)biphenyl-4-yl]meth-(e)-ylidene]butyric acid

HRID 390611노트

반응식

HRID 390611 반응식
[OH-].[Na+].[CH3:3][N:4]([C:13]1[CH:14]=[C:15]([C:19]2[CH:24]=[CH:23][C:22](/[CH:25]=[C:26](\[CH2:32][CH3:33])/[C:27]([O:29]CC)=[O:28])=[CH:21][CH:20]=2)[CH:16]=[CH:17][CH:18]=1)[C:5]([NH:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12])=[O:6]>C(O)C.C(OCC)C>[CH3:3][N:4]([C:13]1[CH:14]=[C:15]([C:19]2[CH:24]=[CH:23][C:22](/[CH:25]=[C:26](\[CH2:32][CH3:33])/[C:27]([OH:29])=[O:28])=[CH:21][CH:20]=2)[CH:16]=[CH:17][CH:18]=1)[C:5]([NH:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12])=[O:6]

참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 68958868Ethyl 2-[1-[3'-(1-methyl-3-pentylureido)biphenyl-4-yl]meth-(e)-ylidene]butyrate

생성물 1

HCID 162244242-[1-[3'-(1-Methyl-3-pentylureido)biphenyl-4-yl]meth-(e)-ylidene]butyric acid수율 84%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 3283Diethyl Ether용매

반응 조건

온도
50 °C

실험 절차

268 mg (6.7 mmol) of sodium hydroxide are added to a solution of 284 mg (0.67 mmol) of ethyl 2-[1-[3′-(1-methyl-3-pentylureido)biphenyl-4-yl]meth-(E)-ylidene]butyrate in 10 mL of ethanol. The reaction mixture is heated at 50° C. for 15 hours. The reaction medium is evaporated to dryness, taken up in water, acidified with 2 N hydrochloric acid solution and extracted with ethyl acetate. The organic phases are combined, washed with water and dried over magnesium sulfate. After filtration, the solvent is evaporated off and the solid obtained is taken up in ethyl ether, filtered off and dried. 222 mg (84%) of 2-[1-[3′-(1-methyl-3-pentylureido)biphenyl-4-yl]meth-(E)-ylidene]butyric acid are obtained in the form of a white powder with a melting point of 150-152° C.

후처리

  1. customThe reaction medium is evaporated to dryness
  2. extractionextracted with ethyl acetate
  3. washwashed with water
  4. dry with materialdried over magnesium sulfate
  5. filtrationAfter filtration
  6. customthe solvent is evaporated off
  7. customthe solid obtained
  8. filtrationfiltered off
  9. customdried

출처 및 근거

ORD 기록
ord-b76868267bfa4044a3186fc5f40b8959
출처 데이터셋
uspto-grants-2013_02
특허 번호
US08383652B2

반응 노트

불러오는 중…